Hydrogen Sulfide → HCID 178506624, compound

HRID 2255353Notes

Reaction equation

HRID 2255353 reaction equation
[OH-:1].[K+:2].[CH2:3]([OH:5])C.[SH2:6].C(=S)=S>O>[C:3](=[S:6])([O-:5])[O-:1].[C:3](=[S:6])([O-:5])[O-:1].[C:3](=[S:6])([O-:5])[O-:1].[C:3](=[S:6])([O-:5])[O-:1].[K+:2].[K+:2].[K+:2].[K+:2].[K+:2].[K+:2].[K+:2].[K+:2]

Participants

6

Reactant 4

HCID 402Hydrogen SulfideHCID 702EthanolHCID 6348Carbon DisulfideHCID 14797Potassium Hydroxide2×

Product 1

HCID 178506624HCID 178506624, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

Twenty grams (0.36 moles) of reagent grade potassium hydroxide was added to 200 grams (255 cc) of absolute ethyl alcohol, with the mixture being refluxed until all of the KOH had dissolved (approximately 1 hour), after which the water formed was removed by a conventional water-alcohol azeotropic distillation. After adding a sufficient amount of absolute alcohol to bring the alcoholic solution back up to about 250 cc and cooling the solution back to room temperature, 5.7 grams (0.18 moles) of finely divided sulfur was added, with stirring, after which 6.1 grams (0.18 moles) of hydrogen sulfide was dissolved therein. At the conclusion of this addition, the temperature of the exothermically heated solution was adjusted to about 130° F. and 13.6 grams (0.19 moles) of carbon disulfide were added, dropwise, thereto over a period of about 30 minutes. The mixture was then heated, under reflux, with stirring, for between about 20 minutes and about 1 hour, after which time a yellow-orange precipitate of potassium tetrathiocarbonate formed. The precipitate was vacuum filtered, under an inert atmosphere, and washed 3 times with about 50 cc of pentane. The washed material was dried, under vacuum, for about 8 hours at 60° C., to produce free-flowing salt particles.

Workup

  1. dissolutionhad dissolved (approximately 1 hour)
  2. customwas removed by a conventional water-alcohol azeotropic distillation
  3. additionAfter adding a sufficient amount of absolute alcohol
  4. addition5.7 grams (0.18 moles) of finely divided sulfur was added
  5. additionAt the conclusion of this addition
  6. customwas adjusted to about 130° F.
  7. temperatureThe mixture was then heated
  8. temperatureunder reflux
  9. stirringwith stirring, for between about 20 minutes and about 1 hour

Sources & evidence

ORD record
ord-0a2b3336a0954dd99d9f25d40e559d92
Source dataset
uspto-grants-1993_08
Patent number
US05240709

Reaction notes

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